Synthesis and Characterization of Nano-Aerogels

Appendices

Appendix 1. American Chemical Society’s Policy on Theses and Dissertations
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Appendix 3. Physical Properties of the Raw Materials Used in This Thesis.

Name	Formula	Molecular weight (g/mol)	Density (g/cm^3)	Purity (%)	Boiling point (°C)	Melting point (°C)
Tetramethyl orthosilicate	C4H12O4Si	152.22	1.032	98	120~122	-4
Tetraethyl orthosilicate	C8H20O4Si	208.33	0.934	98	168	-77
Titanium isopropoxide	C12H28Ti	284.26	0.97	97	240	18-20
Titanium butoxide	C16H36Ti	340.36	1.08	97	310-314	-55
Zirconium propoxide	C12H28Zr	327.58	1.058	70	-	-
Zirconium butoxide	C16H36Zr	383.7	1.049	80	-	-
Aluminum isopropoxide	C9H21Al	204.24	1.035	98	125-130	128-135
Acetic acid	C2H4O2	60.05	1.06	99.7	117.9	16.6
Formic acid	CH2O2	46.03	1.21		100.7	8.3
Benzoic acid	C7H6O2	122.12	1.32	99	248.9	121
Chloroacetic acid	C2H3ClO2	94.50	1.58		188	61-62
Methanol	CH4O	32.04	0.791	99.93	64.7	-98
Ethanol	C2H6O	46.07	0.789	99.95	78.3	-114.1
2-Propanol	C3H8O	60.10	0.785	99.5	82.4	-88.5
n-Butanol	C4H10O	74.12	0.81		117.6	-89.5
Acetone	C3H6O	58.08	0.786	99.5	56.2	-94.3

Appendix 4. Powder XRD Analysis Conditions.

Experimental parameters for Bruker D8 Discover diffractometer

Type of radiation	CuKα1+Kα2 = 1.54184 Å
Power	40 kV x 40 mA
Type of scan	Coupled
Number of frames	3 (merged)
Beam Diameter	500 µm
2θ range	4.9° - 93.95°
Number of samples analyzed	6

Experimental parameters for Rigaku (Rigaku - Geigerflex CN2029) diffractometer

Type of radiation	CuKα1+Kα2 = 1.54184 Å
Power	40 kV x 35 mA
Type of scan	Coupled
Step Size	0.05
Step Time	2sec
2θ range	2.0° - 115.0°
Number of samples analyzed	7

Appendix 5. N₂ Physisorption Analysis Conditions.
Isotherm collection pressure table

	Relative Pressure	BET Surf. area	Lang. Surf. Area	t-Plot	BJH Adsorption	BJH Desorption
1	0.005000000
2	0.010000000			x
3	0.023265306
4	0.030000000			x
5	0.041530612
6	0.059795918
7	0.060000000	x	x	x
8	0.078000000
9	0.080000000	x	x	x
10	0.096326531
11	0.100000000	x	x	x
12	0.114591837
13	0.120000000	x	x	x
14	0.132857143
15	0.140000000	x	x	x	x
16	0.151122449
17	0.160000000	x	x	x	x
18	0.169387755
19	0.180000000	x	x	x	x
20	0.187653061
21	0.200000000	x	x	x	x
22	0.205918367
23	0.224183673
24	0.242448980
25	0.250000000			x	x
26	0.260714286
27	0.278979592
28	0.297244898
29	0.300000000			x	x
30	0.315510204
31	0.333775510
32	0.350000000			x	x
33	0.352040816
34	0.370306122
35	0.388571429
36	0.400000000			x	x
37	0.406836735
38	0.425102041
39	0.443367347
40	0.450000000			x	x
41	0.461632653
42	0.479897959
43	0.498163265
44	0.500000000			x	x
45	0.516428571
46	0.534693878
47	0.550000000			x	x
48	0.552951984
49	0.571224490
50	0.589489796
51	0.600000000			x	x
52	0.607755102
53	0.626020408
54	0.644285714
55	0.650000000			x	x
56	0.662551020
57	0.680816327
58	0.699061633
59	0.700000000				x
60	0.717346939
61	0.735612245
62	0.750000000				x
63	0.753877551
64	0.772142857
65	0.790408163
66	0.800000000				x
67	0.808673469
68	0.820000000				x
69	0.826938776
70	0.845204082
71	0.850000000				x
72	0.863469388
73	0.875000000				x
74	0.881734694
75	0.900000000				x
76	0.925000000				x
77	0.950000000				x
78	0.975000000				x
79	0.980000000				x
80	0.990000000				x
81	0.995000000				x	x
82	0.990000000					x
83	0.980000000					x
84	0.975000000					x
85	0.950000000					x
86	0.925000000					x
87	0.900000000					x
88	0.875000000					x
89	0.850000000					x
90	0.825000000					x
91	0.800000000					x
92	0.750000000					x
93	0.700000000					x
94	0.650000000					x
95	0.600000000					x
96	0.550000000					x
97	0.500000000					x
98	0.450000000					x
99	0.400000000					x
100	0.350000000					x
101	0.300000000					x
102	0.250000000					x
103	0.200000000					x
104	0.140000000					x

Collect ROA Data: No

ROA Sample Interval: 10.00 secs

ROA Dose Amount: 5.00 cm³/g STP

Maximum ROA Samples: 100
Target pressure options:
Use first pressure fixed dose: No

Use maximum volume increment: No

Absolute pressure tolerance: 5.000 mmHg

Relative pressure tolerance: 5.0%

Low pressure dosing: No
Analysis preparation options:
Fast evacuation: Yes

Evacuation time: 0 .10 hours

Leak test: No
Free Space
Free space group: Measured

Low dewar after free space: Yes

Evacuation time: 0.10 hour

Outgas test: Yes

Outgas test duration: 180 secs
Po and Temperature options:
Po type: Measured

Measurement interval: 120 minutes

Temperature type: Entered

Temperature: 77.35 K

Measurement gas: Nitrogen @ 77.35 K (N₂)